Process fob polymerizing



0ct. l5, 19.35.

L. J. REIZENSTEIN PROCESS FOR POLYMERIZING CHINA WOOD OIL Filed Feb. 2. 1932 J6 Je 31% j] so 'm 'E g; I ug1 MA UORNEYS Patented Oct. 15,v 1935 .PATENT OFFICE PROCESS FonjPoLYMEmzmG f clima-woon om Louie J. neuenetem, Pittsburgh. re. Application February 2, 1932, Serial No. 590,389

1 claim. (c1. :x7- 12) 'This invention relates to a process and system for treating'orprocessing China-wood oil and` more specifically to the .polymerization or bodying thereof.'

d As is known, oils like China-wood or tung oil,

which are extensively used in the paint, varnish and lacquer industry are, in their raw state, normally unsaturated, but the molecules of which ratherreadily combine or polymerize, as is understood by those skilled in this art. Such polymerization, however, when the oil is at raised .temperature generally continues rather rapidly once it has started and it is difficult to prevent it from reaching a completely or nearly completely lli` . lacquer industry is undesirable, as such a product Y sion of a continuous closed process and system for polymerized state which in'the paint, varnish and isoinouse.'

Prior to my invention no commercially successe ful process has, so far as I am aware, been developed to a useful degree whereby the desired amount of polymerization can ,be simply secured without substantially exceeding that amount. It has been attempted, for example, to alternately subject oils of this type to a heating medium and then yto the open air but suchv is entirely useless and both ineiective and undependable. Again, the attempt has been made to heat oils of the above type under vacuum while subjecting them in a rather complicated way to a heat exchange apparatus, but such process is not successful and` has not been used commercially as it does not provide a uniform dependable'product which is not a over-polymerized. A s.

By the present invention I have provided a process and system forcontinuously polymerizng China-wood oil and the like under pressure there'- by avoiding all the above noted and other defects and disadvantages and such constitutes one of the objects of the present invention.

Another object of the invention is the provipolymerizing China-wood oil and the like which is simple and eflicient and proportionately successful in practice.

A further object of the invention resides in a process and system for polymerizing China-wood oil and the like by passing the oil in a stream Other and further objects and advantages will be understood by those skilled in this art or will be pointed out hereinafter.

In the accompanying drawing, I Ahave illusl trated schematically a preferred system embody- 5 ing the present invention and in which the present process can be eiiiciently carried out.

Referring first to the drawing in detail the n umeral I0 represents a suitable supply tank or the Y like in which, for example, a large quantity of raw l0 oil to be processed iskept and 4to which, asv desired, fresh oil can be continuously added. The numeral II diagrammatically represents a thermometer of any suitable type by means of which the temperature of the raw oil or, as will be hereinafter apparent, the mixed raw and" partly processed oil can be kept at desired temperature or at a known temperature. At I2, the tank III is suitably provided with lan outlet inwhich is a suitable length of one-inch pipe I3 connecting 20 said tank in the usual manner with the intake side of a pump I4, which may be electrically driven by the motor I5-through shaft I6, or of any other suitable type.- v

From the discharge side of said pump I4 extends 25 the 1" vertical pipe I1 which, at a suitable height, has ,a right-angled bend I8 s o that the pipe is thereafter horizontal and this horizontalpart Il' of the pipe yI1 `extends as shown into a furnace or' heating zone designated generally by thenumeral I 9. 'At the end of the furnace said horizontal pipe hasa return bend 20 which, as shown, may be exposed tothe atmosphere, the pipe thereafter returning at 2| parallel to the pipe I1 and'extending from the furnace or heating zone I9, terminatingin a vertically downwardly extending portion 22 which projects'intoal suitable receiving tank or other receptacle 23.

Just beyond the furnace orieating zone I9, the pipe 2| is provided with a -r-joint 24 extending#o from which is a suitable thermometer 25 which projects down into the pipe and into the oil so as to measure the actual temperature thereof. In practice said thermometer is so arranged that it screws into the T-joint, forming a tight connection. Adjacent this first T-joint 24 is a second T-joint 26 from which extends the by-pass pipe 21 which leads, 'as shown, back into supply tank I0. Bypass pipe 21' is provided as shown with a suitable valve 28 so that the flow through 5.0

the vliy-pass can be increased or diminished at will.

Just prior to the entry of the return pipe 2| into receiving tank or receptacle 23, a needle valve 29 is provided `therein'ior a purpose to be hereinafter explained. Onthe vertical section ,of pipe I1 ex- 55 tending from the discharge side of pump I4 is another T-joint 30 to which is connected a short pipe '3| discharging into supply tank |0 and this section of pipe 3| is provided with a spring-loaded release valve" 32 which may be set to open at a desired pressure and which in the-present case is set to open at about |50 pounds per square inch of pressure. The pipe passing through the furnaceor heating zone is likewise one-inch pipe asin fact, is substantially all the pipe.

i The furnace or heating zone I9 consists of the brickwork 33 supported by suitable beams 'or girders 34 resting upon vertical supports 35. Provided in said yfurnace arethe gas burners 36 which are usedfor heating purposes and these gas burners may readily lbe controlled such as by valves 31. Where the pipe subjected to the heat in the heating zone is one-inch pipe the furnace is preferably about two feet from the top of the brickwork to the bottom of the glrders and this has been found to be a desirable relationship which may, of course, be maintained proportionately when changing either the size of the pipe or the size of the furnace. It is to be understood that the furnace shown is more or less exemplary, but is preferably such that the oil passing therethrough may be rapidly raised in temperature to about five or six hundred degrees fahrenheit, preferably to about 580 F., although this temperature naturally depends upoi various conditions and the particular oil use In operation, assuming that a suilcient supply of raw oil has been placed in supply tank I0, needle valve 29 is closed and pump I4 is started, valve 28 in pipe 21 being open to a greater or lesser extent. The gas burners 36 are now lighted, rapidly imparting their heat to the surroundings and the oil passing through pipes l1'- and 2| becomes quickly heatedin its passage through the furnace and the temperature at whichthe oil leaves the furnace is constantly indicated by the thermometer 25. It is clear that the nrst oil passing through the furnace must seek outlet through pipe 21 since valve 28 is the only one whichis open. :When the thermometer 25 shows that the oil passing from the heating zone is about 580 F. or is at whatever temperature has been predetermined needle valve 29 is gradually opened somewhat and valve 28 is gradually closed.

The pump I4 is of such capacity that it is at all times able to pump into the system much more oil than can be discharged through needle valve' 29 and this results in a considerable pressure being imparted to the oil in the system which in the present instance amounts to about one hundred and fty pounds per square in'ch of pressure and it is clear that the various elements of the system are suitably chosen and/or adjusted to yield this pressure. In order that toomuch pressure may not be imparted to the oil the springloaded release valve 32 is adjusted to open at the optimum pressure desired in the system, 150 lbs.

per square inch, for example, so that if the oil tends to increase in pressure beyond the setting of the spring-loaded release valve such valve will automatically open and allow oil to be discharged back into the supply tank |0 until the pressure Vin the system has again reverted or ,decreased below the release-pressure of the valve. In other words, the spring-loaded release valve is in effect a safety valve.

As will, therefore, be understood from the fore going after the process gets under way and the burners are regulated to give the desired heat and the needle valve regulated to discharge the desired amount the process goes on continu- 5 utilized such .as a suitable water jacket 38 around the discharge elbow to insure that the oil is cooled at least below the ash point or tank 23 can be cooled suitably. a 15 Such oil is found to be rapidly and effectively l prepared from the raw oil and I believe while not limited thereto that the combination of the 'heat and pressure yin some way facilitates the proper polymerization. It is further apparent that the 20 system is subject to close control and that when l once adjusted needs no appreciable attention. Were the oil over polymerized, that is, were the polymerizing action permitted to go to its natural conclusion or end, a product of substantially jellylike or even solid characteristics would be ob- I tained and inasmuch as I do not obtain any of this jelly-like or solid end product I'know that the polymerization has not exceeded the desired extent. 80

It is clear that many of the details hereof are subject to considerable variationwlthout departing from the rspirit and scope of the invention. For example, the maximum temperature may be so chosen that the desired product is secured and, 3l of course,`the temperature depends upon the particular oil being processed and sometimes upon the peculiarities of any given oil. Again, the pressure is subject to considerable variation and the appropriate pressure may be readily se- 0 cured by a suitable adjustment of valve 32. As to the furnace itself the details may be considerably varied provided that relatively rapid and satisfactory heating of the oil is'efiiciently obtained. y 45 It is to be understood that while the invention r has been explained in connection with Chinawood oil or tung oil, it may be used for other I! oils such ashlinseed oil or any organic oil as s animal, vegetable and nsh oils, with any combination of China-wood oil and/or any of such other oils, or for' gums and resins for use in the above connection.

What I claim as newand desire to secure by s Letters Patent is:

The process of polymerizing an unsaturated glyceride oil such as China-wood oil, which comprises maintaining a suitable supply of oil, continuously pumping from the Asupply a stream of o oil through a polymerizing zone, diverting a portion of the oil pumped from the supply back to the supply before reaching the polymerizing zone and creating a constant pressure gradient on the balance thereof in the neighborhood of 65 lbs/sq. in., discharging the oil from the polymerizing zone back to the supply until the oil leaving the -polymerizing zone has attained the ydesired temperature, in the range from 500 to 

